Yarn lubricant



Patented Aug. 21, 1951 YARN LUBRICANT George W. Seymour, Maplewood, andFred Fortess, Summit, N. J., and Marshall Duke, Cumberland, Md.,assignors to Celanese Corporation of America, a corporation of DelawareNo Drawing. Application January 10, 1948, Serial No. 1,663

4 Claims. (01. 252-8.75)

This invention relates to the treatment of textile materials and relatesmore particularly to the lubrication and conditioning of textilematerials such as fibers and filaments having a basis of celluloseacetate or other organic derivative of cellulose.

An object of this invention is the provision of an improved conditioningagent or yarn lubricant for the treatment of textile materials having abasis of cellulose acetate or other organic derivative of cellulose torender the same more amenable to textile operations such as carding,drafting, spinning, twisting, coning, pirning, hanking, weaving,knitting and the like.

Another object of this invention is the provision of an improved textileconditioning agent for yarns, filaments or fibers having a basis ofcellulose acetate or other organic derivative of cellulose materialwhich is stable, resistant to oxidation, and which renders the yarns,filaments or fibers to which it is applied anti-static and readilyadapted to be woven or knitted into fabrics by suitable formingoperations.

Other objects of this invention will appear from the following detaileddescription.

Various compositions comprising vegetable, animal and mineral oils, bothnormal and specially treated, in combination with various othersubstances have been employed for lubricating and conditioning yarns,filaments and fibers having a basis of cellulose acetate or otherorganic derivative of cellulose to render .,the same more amenable tothe several textile operations employed in processing the same intofabrics. These lubricating and conditioning agents reduce the frictionof the yarns against guides and the like and against each other and alsoact to reduce the tendency of said yarns, when moving at very highspeeds during winding and twisting, warping and other textileoperations, to retain undesirably large charges of static electricity.While the use of many of the compositions previouslyemployed hasresulted in a definite improvement in the processing characteristics ofsaid yarns, it has been observed that continued exposure to light andair has a slight tendency to We have now found that the tendency towardoxidation and loss of size adhesion in certain lubricating andconditioning compositions applied to cellulose acetate or other organicderivative of cellulose yarns may be overcome by the use of a novelblended multi-component lubricating and conditioning composition. Thenovel lubricating and conditioning composition of our invention isformed by adding to a mix.- ture of white mineral oil, castor oil, analkylated phenol or other wetting agent, a long chain aliphatic acidsuch as oleic acidand an alkylolamine, which mixture is itself anexcellent lubric'ating and conditioning agent under certain conditions,a suitable amount of the desalted, dehydrated reaction product witholeum of a mixture of a long-chain aliphatic acid, a vegetable oil andmineral oil containing a penetrating agent, which reaction product hasbeen neutralized with an alkali and an alkylolamine prior to saltremoval and dehydration. Where the long-chain aliphatic acid employed inthe initial mixture is oleic acid, it is preferably purified to be lowin linoleic acid. A blending agent such as oleyl alcohol or diglycollaurate may also be present in the mixture to which the salt-free,dehydrated composition is added. The diglycol laurate also exhibitsexcellent humectant and emulsifying properties and is valuable forcontrolling the scourability of the composition. The use of an acylatedvegetable oil in the first-mentioned mixture has also been found to besomewhat advantageous when lubricating or conditioning organic acidester of cellulose yarns.

The white mineral oil employed in forming the novel conditioningmulti-component composition may be one having a parafiinic or naphthenicbase and a viscosity of 50 to seconds. This viscosity and those givenhereinafter are Saybolt Universal at F. However, the viscosity of themineral oil employed is determined by the over-all viscosity desired inthe final conditioning composition or, in other words, the limit ofviscosity of the mineral oil is set by the over-all viscosity of theconditioning composition which can be handled in application. Thisover-all viscosity may be on the order of 80 to 200 seconds andpreferably about seconds. In the mixture comprising our novelconditioning composition, optimum results are obtained using a mineraloil having a parafiinic base and a viscosity of 50 seconds.

The alkylated phenol employed on the present 3 ingredient increases thelubricating value of the oils, reduces the development of static,increases the mutual solubility of th several constituents, lowers theviscosity of the conditioning composition as a whole and improves thewetting power of the same. While we prefer to employ branched chaindiamyl phenols such as di-secondaryor ditertiary-amyl phenol in ourconditioning composition, other alkylated phenols such as a branchedchain dibutyl and di-secondaryand di-tertiary-amyl derivatives ofcresols and xylenols are also advantageously employed. These branchedchain dibutyl and diamyl derivatives may be prepared from any of. theindividual pure cresols and xylenols or from technical grades of mixedcresols and cresylic acids. The branched chain dibutyl and diamylderivatives of any of the mono-chlorophenols may also be satisfactorilyemployed in our novel conditioning composition. The alkylated phenol notonly acts as an anti-oxidant but also governs the penetration and spreadof the conditioning composition in and on the yarn and stabilizes thesame.

These alkylated phenols normally have a compatibility with cellulosederivatives of 1 to 50%, the above diamyl phenols having :acompatibility of about 20%. The compatibility of the phenol derivativesand of acylated vegetable oils with cellulose derivatives is determinedby preparing films of the cellulose derivative and the material orcompound Whose compatibility is being tested. The films are preparedfrom solutions of the cellulose derivative and the phenol or vegetableoil derivative in a suitable volatile solvent, such as acetone, by.pouring said solutions on a glass or metal plate. After the solvent hasevaporated, the film remaining will be clear if the limit ofcompatibility has not been exceeded. The maximum percentage by weightofthe phenol or vegetable oil derivative present in a clear film is thecompatibility.

As stated. above, the presence of an organic ester of vegetable oil inthe initial conditioning fluid mixture to which the desalted, anddehydrated reaction product is added to form the final composition ishighly desirable, particularly when the yarn being treatedis one havinga basis of an organic acid ester of cellulose. Examples of suchvegetable oil organic esters are the formyl, acetyl, propionyl andbutyryl esters of castor oil or castor oil derivatives, specificexamples being acetylated castor oil and butyl acetyl ricinoleate. Theacetylated vegetable oils have a greatly increased degree ofcompatibilitywith the yarn over the unacylated vegetable oils, therebyenhancing the spreading power and wetting out action of the conditioningfluid or dressing. The acetylated vegetable oils may be employed inamounts of from 1 to by weight of the conditioning fluid mixture.

The emulsifiability of the initial fluid mixture to which the salt-free,dehydrated reaction product is added is also improved by the presence ofan amine soap which is preferably formed in the initial fluid mixtureitself by adding thereto a hydroxylated amine, such as triethanolamineor mixed isopropanolamines, and a fatty acid such as oleic acid. Theamine and the fatty acid are preferably added in stoichiometricproportions to form triethanolamine oleate. The amine soap alsocontributes to the anti-static properties of the composition, aids theblending of the components and has a wetting action on cellulose acetateor other organic derivative of cellulose textile materials conditionedwith our novel composition.

In forming the initial fluid mixture, the proportions of the severalcomponents may be varied somewhat depending on the properties it isdesired to emphasize in the treated yarn. Where it is desired toincrease the spreading and wetting properties, the amount of alkylphenol may be increased, where the hand of the yarn is particularlyimportant, the amount of softening agent preesnt should be increased.The mineral oil content of the initial mixture may vary from 50 to 75%by weight.

The de-salted, dehydrated component of our novel lubricating and.conditioning composition, which contains sulfate and/or sulfonategroups, is obtained by reacting a mixture of mineral oil, a vegetableoil such as olive oil, rice oil or peanut oil, and a long chainaliphatic acid such as oleic acid with fuming sulfuric acid such as 20%oleum, at a temperature no greater than about 20 C. Under theseconditions at least part of the aliphatic acid and the vegetable oilemployed are sulfated and/or sulfonated. At the completion of thsulfation and/or sulfonation reaction, an alkylated phenol, such as adibutyl or diamyl phenol is added to the reaction mixture to stabilizethe same and to act as a penetrant and an anti-oxidant. The addition ofthe alkyl phenol is followed by the addition of an alkylolamine, waterand a sufiicient amount of an alkali metal hydroxide to neutralize allof the sulfuric acid remaining and the major portion of the freealiphatic acid. The batch is then stirred until reaction ceases and aclear oil is formed. The process for obtaining this sulfated and/orsulfonated product is more particularly described in U. S. Pat. No.2,406,408. 7

In order to form the improved lubricating and conditioning compositionof the present invention, the sulfated and/ or sulfonated reactionproduct obtained in the manner described above is subjected to ade-salting and dehydration treatment before it is blended with theinitial mixture to form the final lubricating and conditioningcomposition. The de-salting and dehydration is effected by diluting theneutralized reaction product with an organic solvent such as anhydrousisopropyl alcohol which is a nonsolvent for the inorganic salts presentand which forms an azeotrope with water. The alcohol addition causes thesalts to be precipitated from solution. The precipitated salts are thenfiltered out and the isopropyl alcohol distilled off, the water which ispresent in the mixture coming off as an azeotrope with the isopropylalcohol. Preferably, the temperature of the sulfonated mixture beingdistilled should not exceed about 110 C. during the distillationoperation. If any water remains, an additional quantity of anhydrousisopropyl alcohol is then added and the diluted mixture again distilledto remove the remaining water as well as the alcohol. Prior todistillation, a filter aid such as diatomaceous earth or bentonite, forexample, may be added and the solution filtered to improve the clarityand remove any inorganic salts still present. The still residueremaining after distillation comprises the composition employed as thesalt-free, dehydrated component of our novel lubricatin and conditioningcomposition.

To form the lubricating and conditioning composition of our invention,from 1 to 10 parts by weight of the salt-free, dehydrated componentprepared as described above are'added to to Example I The de-salted,dehydrated component of our novel lubricating and conditioningcomposition is prepared as follows:

A mixture of 117 parts by weight of acid-refined white mineral oil ofabout 50 Saybolt viscosity at 100 F., 87 parts by weight of oleic acid,and 43 parts by weight of raw peanut oil are cooled to 8 to 10 C. in asuitable vessel provided with a cooling jacket and then 2'7 parts byweight of 20% oleum are added over a period of onehalf hour. Thetemperature rises due to the exothermic nature of the reaction but themaximum temperature is held to below 25 C. by cooling. The reactionmixture is then stirred for an additional 45 minutes with thetemperature held at 20 C. To the reaction mixture, there are now added21 parts by weight of diamyl phenol, followed by the addition of 4'7parts by weight of triethanolamine, 37 parts by weight of water and 18parts by weight of a 22% by weight aqueous solution of sodium hydroxide.The resulting neutralized mixture is cooled to room temperature withstirring.

The sulfonated reaction mixture obtained is then desalted by theaddition thereto of anhydrous isopropyl alcohol to precipitate theinorganic salts present and the latter are then removed by filtration.The filtered solution is distilled under vacuum and the isopropylalcohol and water are taken off as an azeotropic mixture with the stilltemperature held at a maximum of 110 C. The still residue is dilutedwith an equal volume of anhydrous isopropyl alcohol, about 0.1 to 0.4%by weight of a diatomaceous earth filter aid are added and the mixturefiltered again. The isopropyl alcohol present and any remaining waterare removed by repeating the distillation under vacuum at a maximumstill temperature of 110 C. The still residue comprises the sulfonatedreaction product forming one of the components of my novel lubricatingand conditioning composition.

Example II A fluid mixture is prepared by thoroughly mixing thefollowing components in the proportions given:

Parts by weight Paraifin base white mineral oil (50 seconds viscosity)55.6 Castor oil 18.5 Oleic acid 10.7 Di-tertiary-amyl phenol 9.7Triethanolamine 4.98 Oleyl alcohol 0.55

and to the mixture obtained are added 5 parts by weight of the salt-freedehydrated component obtained in accordance with Example I. Afterfurther mixing, the resulting lubricating and conditioning compositionis ready for use. The

composition has a Saybolt Universal viscosity of about 185 seconds at F.g

Example III A fluid mixture is prepared by thoroughly mixing thefollowing components in the proportions iven:

Parts by weight Parafiln base white mineral oil (50 seconds viscosity)54.5

Castor oil 20 Oleic acid 10.25 Butyl acetyl ricinoleate 5Di-tertiary-amyl phenol 4.5 Triethanolamine 4.75 Oleyl alcohol 1 and tothe mixture obtained are added 5 parts by weight of the salt-free,dehydrated component obtained in accordance with Example I. Afterfurther mixing, the resulting lubricating and conditioning compositionis ready for use. The composition has a Saybolt Universal viscosity ofabout 165 seconds at 100 F.

Example I V A fluid mixture is prepared by thoroughly mixing thefollowing components in the proportions given:

' Parts by weight Parafiin base white mineral oil (50seconds viscosity)55.05 Castor oil 20.2 Oleic acid 10.35 Triethanolamine 4.80 Butyl acetylricinoleate 5.05

Di-tertiary-amyl phenol 4.55

and to the mixture obtained are added 5 parts by weight of thesalt-free, dehydrated component obtained in accordance with Example 1.After further mixing, the resulting lubricating and conditioningcomposition is ready for use. The composition has a Saybolt Universalviscosity of about seconds at 100 F.

Example V A fluid mixture is prepared by thoroughly mixing the followingand to the mixture obtained are added 5 parts by weight of thesalt-free, dehydrated component obtained in accordance with Example I.After further mixing, the resulting lubricating and conditioningcomposition is ready for use. composition has a Saybolt Universalviscosity of about 150 seconds at 100 F. l 1 I L .11

components in the proportions The l Example VI A fluid mixture isprepared by thoroughly mixing the following components in theproportions given:

Parts by weight Paraffin base white mineral oil (50 seconds viscosity)52.38 Castor oil 14. 9 Triethanolamine 4.29 Oleic acid 11.90 Butylacetyl ricinoleate 6.67 Di-tertiary-amyl phenol 5.71

and to the mixture obtained are added 4.7 6 parts by weight of thesalt-free, dehydrated component obtained in accordance with Example I.After further mixing, the resulting lubricating and conditioningcomposition is ready for use. The composition has a Saybolt Universalviscosity of about 150 seconds at 100 F.

Example VII The following components are thoroughly mixed in theproportions given:

. Parts by weight Paraiiin base white mineral oil (50 seconds viscosity)55 Castor oil 15 Di-secondary-amyl phenol 10 Oleic acid 12.5Triethanolamine 4.5

and to the mixture obtained are added 5 parts by weight of thesalt-free, dehydrated component obtained in accordance with Example I.After further mixing, the resulting lubricating and condition ingcomposition is ready for use. The composition has a Saybolt Universalviscosity of 152.1 at 100 F.

Example VIII The following components are thoroughly mixed in theproportions given:

Parts by weight Parafiin base white mineral oil (50 seconds viscosity)Castor oil Oleic acid 12.5 Triethanolamine 4.5 Butyl acetyl ricinoleate'7 Di-secondary-amyl-phenol 6 and to the mixture obtained are added 5parts by weight of the salt-free, dehydrated component obtained inaccordance with Example 1. After further mixing, the resultinglubricating and conditioning composition is ready for use. Thecomposition has a Saybolt Universal viscosity of 146 at 100 F.

Example IX The following components are thoroughly mixed in theproportions given:

and to the mixture obtained are added 5 parts by weight of thesalt-free, dehydrated component obtained in accordance with Example 1.After .further mixing, the resulting lubricating and conditioningcomposition is ready for use. The com- 8 position has a SayboltUniversal viscosity of 149.4 at F.

When applied to yarns, filaments or fibers our novel lubricating andconditioning composition is found to be highly resistant to oxidation,polymerization and gumming even after remaining on the yarns, filamentsor fibers for extended periods prior to the utilization of saidlubricated and conditioned yarns, filaments or fibers for weaving andknitting operations or for yarn formation. Size adherence is found to beexcellent and fraying on the looms due to poor size adhesion iseliminated. In addition, cellulose acetate or other organic derivativeof cellulose yarns lubricated and conditioned with the novel compositionof our invention have substantially improved antistatic properties.

It is to be understood that the foregoing detailed description is givenmerely by way of iilustration and that many variations may be madetherein without departing from the spirit of our invention.

Having described our invention, what we desire to secure by LettersPatent is:

1. A lubricating and conditioning composition for the treatment oftextile materials to render the same more amenable to textileoperations, comprising a mixture of about 55 parts by weight of amineral oil, about 5 to about 12.5 parts by weight of castor oil, 1.5 toabout 5 parts by weight of an alkylolamine, about 5 to about 10 parts byweight of a long chain aliphatic acid, about 5 parts by weight of analkyl phenol and a blending agent selected from the group consisting ofoleyl alcohol and diglycol laurate, said mixture containing 0.01 toabout 0.1 part by weight of said mixture of the de-salted and dehydratedreaction product of oleum with a mixture of a long chain aliphatic acid,a vegetable oil and mineral oil neutralized with an alkali and analkylolamine.

2. A lubricating and conditioning composition for the treatment oftextile materials to render the same more amenable to textileoperations, comprising a mixture of about 55 parts by weight of amineral oil, about 5 to about 12.5 parts by weight of castor oil, 1.5 toabout 5 parts by weight of triethanolamine, about 5 to about 10 parts byweight of oleic acid, about 5 parts by weight of a diamyl phenol and ablending agent selected from the group consisting of oleyl alcohol anddiglycol laurate, said mixture containing 0.01 to about 0.1 part byweight of said mixture of the de-salted and dehydrated reaction productof oleum with a mixture of a long chain aliphatic acid, a vegetable oiland mineral oil neutralized with an alkali and an alkylolamine.

3. A lubricating and conditioning composition for the treatment oftextile materials to render the same more amenable to textileoperations, comprising a mixture of about 55 parts by weight of amineral oil about 5 to about 12.5 parts by weight of castor oil, 1.5 toabout 5 parts by weight of an alkylolamine, about 5 to about 10 parts byWeight of a long chain aliphatic acid, about 5 parts by weight of analkyl phenol and a blending agent selected from the group consisting ofoleyl alcohol and diglycol laurate, said mixture containing 0.01 toabout 0.1 part by weight of said mixture of the de-salted and dehydratedreaction product of oleum with a mixture of oleic acid, peanut oil andmineral oil neutralized with triethanolamine and an aqueous solution ofsodium hydroxide and having a diamyl phenol incorporated therein.

4. A lubricating and conditioning composition for the treatment oftextile materials to render the same more amenable to textileoperations, comprising a mixture of about 55 parts by weight of amineral oil, about 5 to about 12.5 parts by weight of castor oil, 1.5 toabout 5 parts by Weight of triethanolamine, about 5 to about 10 parts byweight of oleic acid, about 5 parts by weight of a diamyl phenol and ablending agent selected from the group consisting of oleyl alcohol anddiglycol laurate, said mixture containing 0.01 to about 0.1 part byweight of said mixture of the de-salted and dehydrated reaction productof oleum with a mixture of oleic acid, peanut oil and mineral oilneutralized with triethanolamine and an aqueous solution of sodiumhydroxide and having a diamyl phenol incorporated therein.

GEORGE W. SEYMOUR. FRED FORTESS. MARSHALL DUKE.

REFERENCES CITED The following references are of record in the file ofthis patent:

UNITED STATES PATENTS

1. A LUBRICATING AND CONDITIONING COMPOSITION FOR THE TREATMENT OFTEXTILE MATERIALS TO RENDER THE SAME MOR AMENABLE TO TEXTILE OPERATIONS,COMPRISING A MIXTURE OF ABOUT 55 PARTS BY WEIGHT OF A MINERAL OIL, ABOUT5 TO ABOUT 12.5 PARTS BY WEIGHT OF CASTOR OIL, 1.5 TO ABOUT 5 PARTS BYOF AN ALKYLOLAMINE, ABOUT 5 TO ABOUT 10 PARTS BY WEIGHT OF A LONG CHAINALIPHATIC ACID, ABOUT 5 PARTS BY WEIGHT OF AN ALKYL PHENOL AND ABLENDING AGENT SELECTED FROM THE GROUP CONSISTING OF OLEYL ALCOHOL ANDDIGLYCOL LAURATE, SAID MIXTURE CONTAINING 0.01 TO ABOUT 0.1 PART BYWEIGHT OF SAID MIXTURE OF THE DE-SALTED AND DEHYDRATED REACTION PRODUCTOF OLEUM WITH A MIXTURE OF A LONG CHAIN ALIPHATIC ACID, A VEGEABLE OILAND MINERAL OIL NEUTRALIZED WITH AN ALKALI AND AN ALKYLOLAMINE.